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1. (WO2005062806) PROCEDE DE PREPARATION DE CATALYSEURS D'OXYDES METALLIQUES MIXTES UTILISES DANS LA PRODUCTION D'ALDEHYDES INSATURES A PARTIR D'OLEFINES
Note: Texte fondé sur des processus automatiques de reconnaissance optique de caractères. Seule la version PDF a une valeur juridique

WHAT IS CLAIMED IS:

1. A process for preparing catalyst for the oxidation of an olefin to an unsaturated aldehyde comprising:

a) dissolving -molybdenum, bismuth, iron, cesium and M compounds in water or acid wherein M is one or more of antimony, phosphorus, boron, sulfur, silicon, aluminum, titanium, tellurium, vanadium, zirconium and niobium;

b) precipitating a catalyst precursor;

c) removing liquid to form a solid;

d) washing the solid;

e) drying the solid;

f) contacting the solid with a solution of M1 compounds wherein M' is one or more selected from cobalt, nickel, magnesium, zinc, potassium, rubidium, thallium, manganese, barium, chromium, cerium, tin, lead, cadmium and copper,

g) drying the solid; and

h) calcining the solid to form oxides of the metals to form a catalyst of the general formula:

Mo12BiaWbFecCsgMmM'm'Ox

wherein a is in the range from 0.1 to 1.5, b is 0 to 9, c is in the range from 0.2 to 5.0, ,g is in the range from 0.1 to 1.5, m is in the range from 0 to 9, m1 is from 0 to 9 and x is determined by the valences of the other components.

2. The process of Claim 1 wherein the molybdenum compound is an ammonium salt.

3. The process of Claim 2 wherein the molybdenum compound is ammonium paramolybdate or ammonium molybdate.

4. The process of Claim 1 wherein the tungsten compound is an ammonium salt.

5. The process of Claim 4 wherein the tungsten compound is ammonium paratungstate or ammonium tungstate.

6-. The process of Claim 1 wherein the bismuth compound is a nitrate.

7. The process of Claim 1 wherein the iron compound is a nitrate.

8. The process of Claim 1 wherein M' is a cobalt compound.

9. The process of Claim .8 wherein the cobalt compound is a nitrate.

10. The process of Claim 1 M' is a nickel compound.

11. The process of Claim 10 wherein the nickel compound is a nitrate.

12. The process of Claim 1 wherein M is an antimony compound.

13. The process of Claim 12 wherein the antimony compound is an oxide.

14. The process of Claim 1 wherein the cesium compound is a nitrate.

15. The process of Claim 1 wherein M' is a zinc compound.

16. The process of Claim 15 wherein the zinc compound is a nitrate.

17. The process of Claim 1 wherein catalyst is of the formula:

Mo12BiaWbFecCodNieSbfCsgMghZniOx

wherein b is 0 to 4, d is 0 to 9, e is 0 to 9, f is 0 to 2.0, h is 0 to 1.5, i is 0 to 2.0.

18. The process of Claim 1 wherein the catalyst has an X-ray diffraction pattern of diffraction peaks at the diffraction angles of 2θ, measured by using Cu Kα radiation, at 9.6, 14.2, 23.0, 26.7 and 28.0 degrees.

19. The process of Claim 1 wherein g is in the range from 0.4 to 1.5.

20. The process of Claim 1 wherein the compounds are dissolved and precipitation occurs at, a .temperature in the range of from 40°C to 100°C.

21. The process of Claim 20 wherein the compounds are dissolved and precipitation occurs at a temperature in the range of from 60°C to 95°C.

22. The process of Claim 1 additionally comprising aging for 2 to 24 hours before the liquid is removed.

23. The process of Claim 22 wherein the aging is for 8 to 18 hours.

24. The process of Claim 23 wherein the aging is for 5 to 10 hours.

25. The process of Claim 1 wherein the solid is calcined at a temperature of 200-600°C for 1-12 hours.

26. The process of Claim 25 wherein the solid is calcined in two stages, one at a temperature of 150-400°C for 1-5 hours and another at a temperature of 460-600°C for 4-8 hours.

27. The process of Claim 26 wherein the two-stage calcination is first at a temperature of 290-310°C for 2 hours and second at a temperature of 460-500°C for 6 hours.

28. The process of Claim 1 wherein the solid is calcined in one stage at a temperature of 450-500°C for 1-4 hours.

29. The process of Claim 27 wherein the temperature is increased from the first stage to the second stage at 0.5 to 20°C/min.

30. The process of Claim 29 wherein the temperature is increased at 5 to 10°C/min.

31. The process of Claim 28 wherein the temperature is increased from ambient to the calcination temperature at 0.5 to 20°C/min.

32. The process of Claim 31 wherein the temperature is increased at 5 to 10°C/min.